#------------------------------------------------------------------------------
#$Date: 2024-08-07 01:06:36 +0300 (Wed, 07 Aug 2024) $
#$Revision: 294001 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/31/2023161.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2023161
loop_
_publ_author_name
'Babu, Sainath'
'Fronczek, Frank R.'
'Uppu, Rao M.'
'Claville, Michelle O.'
_publ_section_title
;
Crystal structures of the isomeric dipeptides l-glycyl-l-me-thio-nine and
l-me-thionyl-l-glycine.
;
_journal_coeditor_code HB8099
_journal_issue 'Pt 7'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first 725
_journal_page_last 728
_journal_paper_doi 10.1107/S2056989024005504
_journal_volume 80
_journal_year 2024
_chemical_absolute_configuration rmad
_chemical_formula_iupac 'C7 H14 N2 O3 S'
_chemical_formula_moiety 'C7 H14 N2 O3 S'
_chemical_formula_sum 'C7 H14 N2 O3 S'
_chemical_formula_weight 206.26
_chemical_name_systematic
;
L-Glycyl-L-methionine
;
_space_group_crystal_system monoclinic
_space_group_IT_number 4
_space_group_name_Hall 'P 2yb'
_space_group_name_H-M_alt 'P 1 21 1'
_atom_sites_solution_hydrogens mixed
_audit_creation_method SHELXL-2018/1
_cell_angle_alpha 90
_cell_angle_beta 91.147(4)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 6.2517(2)
_cell_length_b 5.4935(2)
_cell_length_c 14.5686(6)
_cell_measurement_reflns_used 5067
_cell_measurement_temperature 90.0(5)
_cell_measurement_theta_max 40.05
_cell_measurement_theta_min 2.80
_cell_volume 500.24(3)
_computing_cell_refinement
;
SAINT (Bruker, 2016)
;
_computing_data_collection
;
APEX2 (Bruker, 2016)
;
_computing_data_reduction
;
SAINT (Bruker, 2016)
;
_computing_molecular_graphics
;
Mercury (Macrae et al., 2020)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2018/1 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature 90.0(5)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type 'Bruker Kappa APEXII DUO CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator 'TRIUMPH curved graphite'
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0257
_diffrn_reflns_av_unetI/netI 0.0415
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_k_min -9
_diffrn_reflns_limit_l_max 26
_diffrn_reflns_limit_l_min -26
_diffrn_reflns_number 11393
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 40.266
_diffrn_reflns_theta_min 2.797
_exptl_absorpt_coefficient_mu 0.303
_exptl_absorpt_correction_T_max 0.9910
_exptl_absorpt_correction_T_min 0.8356
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.369
_exptl_crystal_description plate
_exptl_crystal_F_000 220
_exptl_crystal_size_max 0.380
_exptl_crystal_size_mid 0.290
_exptl_crystal_size_min 0.030
_refine_diff_density_max 0.532
_refine_diff_density_min -0.303
_refine_ls_abs_structure_details
;
Flack x determined using 2141 quotients
[(I^+^)-(I^-^)]/[(I^+^)+(I^-^)]
Parsons et al. (2013)
;
_refine_ls_abs_structure_Flack 0.02(2)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.044
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 131
_refine_ls_number_reflns 5922
_refine_ls_number_restraints 1
_refine_ls_restrained_S_all 1.044
_refine_ls_R_factor_all 0.0399
_refine_ls_R_factor_gt 0.0332
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0417P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0756
_refine_ls_wR_factor_ref 0.0792
_reflns_number_gt 5356
_reflns_number_total 5922
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file hb8099.cif
_cod_data_source_block Gly-Met
_cod_depositor_comments
'Adding full bibliography for 2023161--2023162.cif.'
_cod_original_sg_symbol_H-M 'P 21'
_cod_database_code 2023161
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min 0.894
_shelx_estimated_absorpt_t_max 0.991
_shelx_hkl_file
;
-2 0 0 619.11 16.82
-3 0 0 36.79 1.01
3 0 0 37.65 1.01
-3 0 0 35.76 1.07
-3 0 0 32.33 1.13
-4 0 0 9.62 0.39
-4 0 0 9.24 0.49
4 0 0 8.90 0.43
-5 0 0 73.93 2.26
5 0 0 72.05 2.00
-5 0 0 70.91 2.01
-6 0 0 35.44 1.31
6 0 0 34.22 1.20
7 0 0 0.06 0.24
8 0 0 35.16 1.37
9 0 0 22.83 1.13
10 0 0 40.60 1.68
11 0 0 6.59 0.82
0 -1 0 -0.25 0.10
0 1 0 -0.37 0.10
1 -1 0 48.38 1.42
1 -1 0 48.30 1.17
-1 1 0 44.47 1.43
2 -1 0 32.32 1.07
2 1 0 34.11 0.90
-3 -1 0 73.50 2.00
3 -1 0 72.62 1.90
3 1 0 76.22 1.88
3 1 0 75.45 1.95
-3 1 0 71.88 2.23
4 -1 0 32.61 1.01
-4 1 0 33.97 1.21
4 1 0 33.48 0.94
-4 1 0 33.99 1.05
4 1 0 35.44 1.07
5 -1 0 15.09 0.63
-5 -1 0 14.91 0.67
-5 1 0 15.12 0.75
-5 1 0 15.41 0.63
5 1 0 15.79 0.68
6 -1 0 38.53 1.31
-6 -1 0 41.88 1.44
-6 1 0 41.85 1.53
6 1 0 42.48 1.39
7 -1 0 3.92 0.44
-7 1 0 4.76 0.55
7 1 0 4.25 0.48
8 -1 0 0.83 0.34
8 1 0 0.75 0.34
9 -1 0 12.70 0.83
9 1 0 11.55 0.86
10 -1 0 6.01 0.69
10 1 0 5.42 0.72
11 -1 0 3.77 0.65
11 1 0 4.48 0.69
0 -2 0 337.67 9.13
0 2 0 324.62 9.11
-1 -2 0 114.00 3.16
1 2 0 106.97 2.79
2 -2 0 331.33 8.22
-2 -2 0 348.17 8.33
-2 -2 0 340.05 8.29
-2 2 0 350.62 8.27
-2 2 0 336.03 9.53
2 2 0 351.23 8.32
2 2 0 349.82 8.29
3 -2 0 11.88 0.39
-3 -2 0 12.45 0.54
3 -2 0 11.78 0.46
-3 -2 0 12.09 0.53
-3 2 0 11.49 0.61
3 2 0 12.31 0.53
-3 2 0 12.20 0.43
3 2 0 12.05 0.49
-4 -2 0 19.85 0.76
4 -2 0 20.63 0.63
4 -2 0 20.80 0.71
4 2 0 20.40 0.78
-4 2 0 19.38 0.60
4 2 0 19.42 0.69
-4 2 0 19.86 0.89
5 -2 0 20.61 0.77
5 -2 0 20.26 0.67
-5 -2 0 20.44 0.81
-5 2 0 19.60 0.79
-5 2 0 18.56 0.92
5 2 0 19.45 0.83
5 2 0 19.37 0.71
6 -2 0 43.95 1.40
-6 2 0 44.32 1.67
6 2 0 42.64 1.48
-6 2 0 43.93 1.45
7 -2 0 11.71 0.68
-7 2 0 12.37 0.83
7 2 0 11.74 0.76
8 -2 0 13.11 0.79
8 2 0 14.69 0.91
9 -2 0 10.35 0.79
9 2 0 11.76 0.90
10 -2 0 5.37 0.67
10 2 0 4.75 0.70
11 -2 0 0.26 0.41
11 2 0 0.25 0.44
0 -3 0 -0.10 0.12
0 3 0 0.10 0.16
0 3 0 -0.04 0.13
1 -3 0 6.40 0.34
-1 -3 0 6.25 0.37
1 3 0 5.68 0.34
-1 3 0 5.36 0.41
-1 3 0 5.76 0.37
1 3 0 5.55 0.38
2 -3 0 25.03 0.79
-2 -3 0 25.83 0.86
2 3 0 24.31 0.83
-2 3 0 23.65 0.81
2 3 0 23.84 0.85
3 -3 0 12.70 0.51
-3 -3 0 12.34 0.59
3 3 0 11.62 0.56
-3 3 0 12.15 0.51
-3 3 0 12.65 0.69
3 3 0 11.98 0.57
-4 -3 0 25.02 0.94
4 -3 0 25.80 0.85
4 3 0 24.63 0.89
-4 3 0 24.03 0.79
4 3 0 22.98 0.91
-4 3 0 23.72 1.07
5 -3 0 5.65 0.43
-5 -3 0 5.62 0.50
5 3 0 5.97 0.53
5 3 0 5.34 0.45
-5 3 0 4.62 0.56
6 -3 0 15.50 0.73
-6 3 0 13.68 0.74
6 3 0 14.17 0.81
-6 3 0 14.08 0.89
7 -3 0 1.99 0.37
-7 3 0 2.34 0.48
7 3 0 1.41 0.38
8 -3 0 5.20 0.57
8 3 0 5.39 0.64
9 -3 0 2.31 0.46
9 3 0 2.18 0.52
10 -3 0 8.13 0.79
10 3 0 7.99 0.90
0 -4 0 129.05 3.40
0 4 0 130.60 3.47
0 4 0 135.61 3.37
1 -4 0 37.89 1.16
-1 -4 0 36.98 1.18
1 4 0 37.27 1.15
-1 4 0 35.30 1.36
-1 4 0 35.79 1.20
-2 -4 0 33.12 1.12
2 -4 0 33.52 1.06
2 4 0 35.57 1.11
-2 4 0 33.39 1.11
-2 4 0 26.22 1.25
2 4 0 34.95 1.16
3 -4 0 31.41 1.01
-3 -4 0 31.42 1.10
-3 4 0 29.17 1.02
3 4 0 29.68 1.09
3 4 0 29.23 1.06
-3 4 0 29.50 1.25
-4 -4 0 0.44 0.25
4 -4 0 0.64 0.21
-4 4 0 -0.09 0.23
-4 4 0 0.27 0.18
4 4 0 -0.09 0.21
4 4 0 0.49 0.24
5 -4 0 48.77 1.55
-5 -4 0 50.69 1.67
5 4 0 49.26 1.67
5 4 0 49.39 1.61
-5 4 0 49.45 1.93
6 -4 0 0.91 0.30
-6 4 0 1.77 0.44
-6 4 0 1.25 0.34
6 4 0 0.43 0.30
7 -4 0 21.25 1.00
-7 4 0 21.89 1.27
-7 4 0 23.37 1.15
7 4 0 21.75 1.13
8 -4 0 29.41 1.24
8 4 0 29.36 1.40
9 -4 0 8.84 0.77
9 4 0 12.14 0.98
10 -4 0 3.23 0.58
10 4 0 3.85 0.69
0 -5 0 -0.13 0.18
0 5 0 -0.17 0.22
-1 -5 0 44.77 1.44
1 -5 0 43.25 1.41
1 5 0 44.16 1.38
-1 5 0 43.32 1.47
1 5 0 44.17 1.49
-2 -5 0 52.31 1.70
2 -5 0 54.06 1.63
2 5 0 51.61 1.72
-2 5 0 52.07 1.68
-2 5 0 53.41 1.96
2 5 0 55.52 1.66
-3 -5 0 12.53 0.72
3 -5 0 11.55 0.62
3 5 0 11.14 0.66
-3 5 0 10.94 0.63
-3 5 0 10.89 0.78
3 5 0 10.35 0.69
-4 -5 0 97.25 2.79
4 -5 0 93.22 2.64
4 5 0 91.70 2.76
-4 5 0 93.50 2.64
4 5 0 96.50 2.76
-4 5 0 94.92 3.22
-5 -5 0 4.38 0.55
5 -5 0 4.22 0.46
-5 5 0 5.34 0.69
5 5 0 3.98 0.50
5 5 0 4.40 0.53
6 -5 0 25.51 1.12
6 5 0 27.96 1.21
6 5 0 26.42 1.23
7 -5 0 10.39 0.75
-7 5 0 11.09 0.86
7 5 0 10.88 0.88
8 -5 0 0.97 0.36
8 5 0 0.84 0.44
9 -5 0 7.92 0.79
9 5 0 6.77 0.83
0 -6 0 1.65 0.35
0 6 0 1.05 0.34
1 -6 0 1.44 0.32
-1 -6 0 1.01 0.31
1 6 0 1.20 0.36
-1 6 0 1.51 0.36
-2 -6 0 16.58 0.89
2 -6 0 14.75 0.80
2 6 0 15.75 0.90
2 6 0 17.11 0.82
-2 6 0 15.65 0.86
-3 -6 0 21.43 1.03
3 -6 0 19.04 0.92
3 6 0 20.07 0.96
-3 6 0 20.65 1.18
3 6 0 20.57 1.04
-3 6 0 20.68 0.98
4 -6 0 5.35 0.55
-4 -6 0 5.58 0.62
4 6 0 4.98 0.56
4 6 0 5.21 0.60
-4 6 0 4.36 0.69
-4 6 0 5.43 0.53
5 -6 0 1.76 0.39
-5 -6 0 2.38 0.51
5 6 0 1.30 0.41
5 6 0 1.78 0.43
6 -6 0 19.79 1.02
6 6 0 17.98 1.10
6 6 0 18.80 1.10
7 -6 0 14.52 0.93
-7 6 0 16.23 1.08
7 6 0 16.54 1.10
8 -6 0 8.29 0.80
8 6 0 8.10 0.93
9 -6 0 2.76 0.55
9 6 0 2.42 0.65
0 -7 0 -0.22 0.26
0 7 0 -0.08 0.33
1 -7 0 9.63 0.75
-1 -7 0 9.63 0.76
-1 7 0 9.78 0.79
1 7 0 10.41 0.82
2 -7 0 12.16 0.80
-2 -7 0 10.77 0.84
2 7 0 11.99 0.89
-2 7 0 13.09 0.87
3 -7 0 8.89 0.71
-3 -7 0 7.33 0.73
3 7 0 8.82 0.83
-3 7 0 7.40 0.72
4 -7 0 8.75 0.73
-4 -7 0 9.78 0.89
4 7 0 10.58 0.92
5 -7 0 0.29 0.34
-5 -7 0 0.58 0.44
5 7 0 0.45 0.38
5 7 0 0.65 0.44
6 -7 0 15.21 0.96
6 7 0 14.60 1.06
6 7 0 14.26 1.07
7 -7 0 0.61 0.42
-7 7 0 0.45 0.44
7 7 0 1.06 0.48
8 -7 0 3.74 0.63
8 7 0 2.53 0.67
0 -8 0 2.00 0.50
0 8 0 1.62 0.51
-1 -8 0 0.74 0.41
1 -8 0 0.46 0.37
-1 8 0 0.25 0.39
1 8 0 0.87 0.43
-2 -8 0 13.02 0.98
2 -8 0 12.80 0.92
2 8 0 13.80 1.05
-2 8 0 12.36 0.99
3 -8 0 2.53 0.51
-3 -8 0 1.88 0.53
-3 8 0 1.97 0.53
3 8 0 3.08 0.64
4 -8 0 0.01 0.36
-4 -8 0 0.72 0.48
4 8 0 1.00 0.48
-5 -8 0 9.33 1.01
5 -8 0 6.61 0.74
5 8 0 7.64 0.90
6 -8 0 4.82 0.69
6 8 0 5.61 0.82
0 -9 0 0.90 0.45
0 9 0 -0.16 0.45
-1 -9 0 12.64 1.04
1 -9 0 14.15 1.05
1 9 0 13.57 1.11
-1 9 0 14.18 1.17
-2 -9 0 24.47 1.41
2 -9 0 21.78 1.23
2 9 0 22.14 1.38
-2 9 0 22.25 1.36
-3 -9 0 4.28 0.72
3 -9 0 3.96 0.64
-3 9 0 5.19 0.75
3 9 0 3.81 0.72
4 -9 0 19.09 1.20
-4 -9 0 21.76 1.40
4 9 0 20.98 1.39
11 0 -1 1.26 0.53
10 0 -1 0.09 0.36
9 0 -1 1.75 0.43
8 0 -1 3.41 0.48
-7 0 1 10.93 0.71
7 0 -1 9.99 0.67
-6 0 1 1.33 0.29
6 0 -1 0.82 0.26
5 0 -1 7.74 0.47
-5 0 1 8.25 0.53
-4 0 1 171.96 4.85
-4 0 1 167.98 4.34
4 0 -1 169.54 4.24
3 0 -1 -0.14 0.12
-3 0 1 -0.10 0.11
1 0 1 47.04 1.31
-1 0 -1 46.15 1.31
-2 0 -1 120.38 3.06
-2 0 -1 115.72 3.30
-3 0 -1 0.58 0.17
-3 0 -1 0.80 0.16
-3 0 -1 0.90 0.15
3 0 1 0.61 0.14
-4 0 -1 5.31 0.40
4 0 1 4.69 0.31
-4 0 -1 4.70 0.34
-4 0 -1 4.41 0.28
-5 0 -1 34.07 1.10
-5 0 -1 36.13 1.24
5 0 1 36.09 1.12
-6 0 -1 2.41 0.35
6 0 1 1.88 0.31
7 0 1 8.78 0.61
8 0 1 0.04 0.27
9 0 1 1.97 0.46
10 0 1 2.54 0.52
11 0 1 -0.01 0.40
11 -1 -1 6.17 0.77
11 1 -1 5.13 0.76
10 -1 -1 7.23 0.79
10 1 -1 7.21 0.79
9 -1 -1 12.27 0.84
9 1 -1 11.59 0.86
8 -1 -1 2.52 0.43
8 1 -1 2.37 0.44
7 -1 -1 21.66 0.95
7 1 -1 21.52 0.98
-7 1 1 21.29 1.06
-6 -1 1 18.46 0.85
6 -1 -1 18.68 0.80
6 1 -1 18.89 0.85
-6 1 1 19.85 0.94
-5 -1 1 28.74 0.99
5 -1 -1 28.43 0.97
5 1 -1 28.05 1.01
-5 1 1 29.75 0.95
-5 1 1 29.05 1.15
4 -1 -1 227.23 5.66
-4 -1 1 233.33 5.69
4 1 -1 241.59 5.59
-4 1 1 214.27 5.89
-4 1 1 234.56 6.54
4 1 -1 230.32 5.69
3 -1 -1 9.71 0.41
3 1 -1 9.52 0.38
3 1 -1 9.93 0.43
-3 1 1 9.01 0.50
2 -1 -1 547.50 12.71
2 -1 -1 522.79 14.58
2 1 -1 530.01 12.71
1 -1 -1 131.50 3.11
1 -1 -1 127.71 3.61
1 1 -1 126.35 3.14
0 -1 -1 410.89 11.21
0 -1 1 423.10 11.23
0 1 1 402.39 11.20
1 -1 1 1000.00 26.60
-1 1 -1 957.60 26.62
-2 -1 -1 38.59 1.10
2 -1 1 38.84 1.22
-2 1 -1 38.58 1.22
2 1 1 38.91 1.03
-3 -1 -1 24.86 0.84
3 -1 1 26.24 0.74
-3 1 -1 24.60 0.90
3 1 1 24.22 0.71
-3 1 -1 24.47 0.82
3 1 1 25.33 0.79
-3 1 -1 25.83 0.82
4 -1 1 58.92 1.59
-4 -1 -1 55.04 1.71
4 1 1 59.78 1.52
-4 1 -1 58.00 1.87
4 1 1 59.46 1.65
-4 1 -1 61.26 1.71
5 -1 1 1.02 0.21
-5 -1 -1 1.16 0.22
-5 1 -1 0.74 0.24
5 1 1 0.87 0.23
-5 1 -1 0.50 0.18
6 -1 1 64.48 1.87
-6 -1 -1 66.80 2.05
-6 1 -1 62.82 2.14
-6 1 -1 64.88 1.93
6 1 1 65.30 1.94
7 -1 1 15.87 0.75
7 1 1 14.21 0.80
-7 1 -1 16.44 0.86
8 -1 1 22.19 1.02
8 1 1 24.91 1.11
9 -1 1 1.80 0.41
9 1 1 1.15 0.40
10 -1 1 9.94 0.82
10 1 1 8.57 0.85
11 -1 1 8.94 0.88
11 1 1 6.75 0.83
11 -2 -1 7.20 0.83
11 2 -1 6.07 0.82
10 -2 -1 10.15 0.88
10 2 -1 10.37 0.97
9 -2 -1 7.23 0.71
9 2 -1 7.21 0.77
8 -2 -1 12.22 0.77
8 2 -1 12.92 0.87
7 -2 -1 1.41 0.31
7 2 -1 0.23 0.26
-7 2 1 0.67 0.34
6 -2 -1 2.43 0.35
-6 2 1 2.33 0.41
6 2 -1 2.74 0.39
-6 2 1 2.81 0.34
5 -2 -1 74.18 1.98
5 -2 -1 71.57 2.07
-5 -2 1 73.90 2.11
-5 2 1 77.28 2.15
-5 2 1 74.95 2.45
5 2 -1 75.54 2.01
5 2 -1 71.19 2.13
-4 -2 1 3.51 0.35
4 -2 -1 3.50 0.26
4 -2 -1 3.57 0.31
4 2 -1 3.28 0.30
4 2 -1 3.76 0.36
-4 2 1 3.31 0.40
3 -2 -1 53.03 1.40
-3 -2 1 53.44 1.52
3 -2 -1 53.57 1.46
3 2 -1 54.98 1.53
-3 2 1 51.18 1.75
3 2 -1 54.62 1.49
2 -2 -1 71.48 1.82
2 -2 -1 71.04 1.87
-2 -2 1 73.52 1.93
-2 2 1 72.08 2.22
2 2 -1 75.47 1.93
2 2 -1 73.52 1.93
-1 -2 1 106.91 2.69
1 -2 -1 108.74 2.67
-1 2 1 103.93 3.09
1 2 -1 108.30 2.72
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9 1 9 8.55 0.73
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4 2 -9 11.65 0.66
3 -2 -9 88.86 2.57
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1 3 -21 29.42 1.48
1 3 -21 28.53 1.41
0 -3 21 1.88 0.43
0 -3 -21 1.57 0.55
0 3 -21 1.86 0.52
0 3 -21 1.85 0.51
-1 -3 -21 4.78 0.74
1 -3 21 5.08 0.56
-1 3 -21 6.03 0.82
-1 3 -21 5.73 0.77
-1 3 -21 4.75 0.68
-2 -3 -21 1.69 0.56
-2 3 -21 2.23 0.66
-2 3 -21 2.60 0.57
-2 3 -21 1.26 0.47
-3 -3 -21 4.74 0.78
-3 3 -21 5.25 0.85
-3 3 -21 6.57 0.79
-4 -3 -21 1.66 0.63
-4 3 -21 1.31 0.51
-4 3 -21 0.78 0.62
-5 -3 -21 3.71 0.79
-5 3 -21 3.84 0.85
-5 -4 21 1.78 0.60
-4 -4 21 2.54 0.58
4 -4 -21 2.67 0.65
4 4 -21 2.79 0.66
-3 -4 21 11.00 0.92
3 -4 -21 11.34 1.06
3 4 -21 10.61 1.03
2 -4 -21 3.37 0.67
-2 -4 21 3.23 0.56
2 4 -21 2.86 0.61
-1 -4 21 10.64 0.84
1 -4 -21 9.39 0.96
1 4 -21 9.77 0.99
0 -4 -21 6.34 0.84
0 -4 21 6.05 0.65
0 4 -21 8.65 0.93
-1 -4 -21 0.95 0.55
1 -4 21 0.69 0.34
-1 4 -21 2.13 0.59
-1 4 -21 1.36 0.54
-2 -4 -21 2.52 0.68
-2 4 -21 2.35 0.67
-2 4 -21 3.21 0.65
-3 -4 -21 3.49 0.73
-3 4 -21 4.36 0.81
-4 -4 -21 0.68 0.55
-4 4 -21 -0.12 0.51
-5 -4 -21 7.88 0.98
-4 -5 21 7.54 0.89
-3 -5 21 5.21 0.73
3 5 -21 5.87 0.85
-2 -5 21 3.81 0.62
2 5 -21 3.42 0.67
-1 -5 21 5.75 0.72
1 -5 -21 6.70 0.90
1 5 -21 5.91 0.82
0 -5 21 0.58 0.42
0 -5 -21 0.87 0.54
0 5 -21 0.63 0.49
-1 -5 -21 9.92 1.05
-1 5 -21 9.39 0.99
-1 5 -21 7.74 0.97
-2 -5 -21 0.56 0.57
-2 5 -21 0.55 0.55
-3 -5 -21 0.10 0.56
-3 5 -21 -0.09 0.53
-1 -6 21 0.45 0.46
0 -6 21 7.62 0.77
-6 0 22 13.82 1.17
-5 0 22 5.32 0.75
-4 0 22 0.99 0.45
3 0 -22 0.11 0.42
2 0 -22 2.75 0.60
2 0 -22 1.88 0.57
1 0 -22 0.22 0.40
1 0 -22 0.69 0.51
0 0 -22 1.30 0.52
-1 0 -22 -0.33 0.38
-2 0 -22 18.67 1.25
-3 0 -22 11.32 1.08
-4 0 -22 16.86 1.30
-5 0 -22 2.51 0.68
-6 0 -22 0.37 0.50
-6 -1 22 4.16 0.75
-6 1 22 2.38 0.66
-5 -1 22 2.37 0.57
-5 1 22 1.50 0.53
-4 -1 22 4.50 0.68
3 -1 -22 1.77 0.54
-3 -1 22 2.53 0.51
3 1 -22 2.05 0.57
2 -1 -22 18.87 1.24
2 -1 -22 21.20 1.27
2 1 -22 20.98 1.21
2 1 -22 22.27 1.32
1 -1 -22 7.26 0.86
1 1 -22 6.85 0.88
1 1 -22 8.61 0.89
0 -1 -22 2.66 0.60
0 1 -22 1.64 0.55
-1 -1 -22 6.62 0.84
-1 1 -22 9.13 0.92
-2 -1 -22 2.06 0.58
-2 1 -22 2.72 0.63
-3 -1 -22 2.88 0.67
-3 1 -22 3.12 0.69
-4 -1 -22 10.52 1.10
-4 1 -22 9.20 1.06
-5 -1 -22 2.73 0.67
-5 1 -22 1.46 0.63
-6 -1 -22 1.41 0.58
-6 1 -22 1.30 0.60
-6 -2 22 2.22 0.59
-6 2 22 2.63 0.68
-5 -2 22 16.33 1.17
-4 -2 22 0.02 0.39
4 2 -22 -0.25 0.44
-3 -2 22 10.91 0.91
3 2 -22 10.51 1.01
3 2 -22 9.94 1.04
2 -2 -22 5.73 0.80
-2 -2 22 6.06 0.68
2 2 -22 7.15 0.86
2 2 -22 7.87 0.85
2 2 -22 5.72 0.75
1 -2 -22 4.11 0.70
-1 -2 22 5.10 0.61
1 2 -22 4.73 0.69
1 2 -22 4.59 0.68
1 2 -22 4.48 0.69
0 -2 -22 12.49 1.04
0 -2 22 11.88 0.83
0 2 -22 12.64 1.01
0 2 -22 11.66 1.00
-1 -2 -22 2.22 0.60
-1 2 -22 2.10 0.54
-2 -2 -22 -0.34 0.39
-2 2 -22 0.73 0.47
-3 -2 -22 1.18 0.55
-3 2 -22 1.33 0.58
-4 -2 -22 1.04 0.57
-4 2 -22 0.06 0.49
-5 -2 -22 0.47 0.55
-5 2 -22 0.79 0.57
-5 -3 22 10.14 1.03
5 3 -22 8.07 0.94
-4 -3 22 5.84 0.79
4 3 -22 4.91 0.79
3 -3 -22 -0.02 0.46
-3 -3 22 0.05 0.38
3 3 -22 0.07 0.47
-2 -3 22 1.31 0.44
2 -3 -22 -0.07 0.45
2 3 -22 0.56 0.48
2 3 -22 0.44 0.45
1 -3 -22 3.09 0.64
-1 -3 22 3.69 0.58
1 3 -22 3.01 0.67
1 3 -22 2.10 0.57
0 -3 22 2.09 0.47
0 -3 -22 0.96 0.49
0 3 -22 1.26 0.53
0 3 -22 0.89 0.49
-1 -3 -22 9.55 1.01
1 -3 22 9.42 0.76
-1 3 -22 10.91 0.98
-1 3 -22 12.00 0.99
-2 -3 -22 2.16 0.65
-2 3 -22 3.13 0.63
-3 -3 -22 2.07 0.66
-3 3 -22 1.81 0.55
-4 -3 -22 4.66 0.85
-5 -3 -22 2.92 0.78
-4 -4 22 2.42 0.61
4 -4 -22 2.77 0.68
4 4 -22 2.05 0.72
-3 -4 22 17.85 1.15
3 -4 -22 16.60 1.26
3 4 -22 16.98 1.25
2 -4 -22 1.32 0.57
-2 -4 22 1.67 0.48
2 4 -22 1.70 0.57
-1 -4 22 2.18 0.49
1 -4 -22 3.15 0.66
1 4 -22 2.89 0.65
0 -4 22 1.53 0.43
0 -4 -22 2.03 0.58
0 4 -22 1.13 0.54
-1 -4 -22 3.92 0.75
-1 4 -22 2.40 0.64
-1 4 -22 3.11 0.72
-2 -4 -22 4.53 0.81
-2 4 -22 6.47 0.83
-2 4 -22 4.65 0.82
-3 -4 -22 -0.79 0.47
-3 4 -22 -0.75 0.49
-4 -4 -22 7.24 0.94
-2 -5 22 4.66 0.71
-1 -5 22 1.44 0.47
1 5 -22 1.50 0.58
0 -5 22 10.33 0.90
0 -5 -22 10.45 1.07
0 5 -22 10.22 1.05
-1 -5 -22 2.08 0.63
-1 5 -22 1.47 0.58
-2 -5 -22 1.68 0.65
-2 5 -22 0.86 0.61
-5 0 23 1.71 0.58
-4 0 23 6.61 0.78
2 0 -23 0.70 0.48
2 0 -23 -0.02 0.42
1 0 -23 11.73 1.03
1 0 -23 10.65 0.99
0 0 -23 34.37 1.69
-1 0 -23 2.39 0.62
-2 0 -23 13.57 1.17
-3 0 -23 3.61 0.76
-4 0 -23 2.82 0.73
-5 0 -23 5.55 0.91
-5 -1 23 1.69 0.59
-5 1 23 3.01 0.67
-4 -1 23 16.94 1.14
-3 -1 23 3.71 0.65
2 -1 -23 10.78 1.09
2 1 -23 11.00 1.06
2 1 -23 12.17 1.05
1 -1 -23 1.04 0.53
1 1 -23 1.66 0.53
1 1 -23 0.82 0.49
0 -1 -23 3.48 0.65
0 1 -23 4.23 0.72
-1 -1 -23 2.04 0.59
-1 1 -23 1.90 0.59
-2 -1 -23 3.67 0.72
-2 1 -23 2.33 0.61
-3 -1 -23 3.26 0.71
-3 1 -23 2.63 0.68
-4 -1 -23 -0.15 0.47
-4 1 -23 0.59 0.58
-5 -1 -23 0.88 0.58
-5 1 -23 1.75 0.65
-5 -2 23 1.61 0.56
-4 -2 23 1.36 0.51
3 -2 -23 6.51 0.89
-3 -2 23 4.01 0.64
2 -2 -23 0.44 0.54
-2 -2 23 0.55 0.39
2 2 -23 0.26 0.47
-1 -2 23 13.80 0.94
1 -2 -23 13.03 1.14
1 2 -23 14.46 1.17
0 -2 -23 2.91 0.64
0 -2 23 1.76 0.45
0 2 -23 1.99 0.58
1 -2 23 2.79 0.47
-1 -2 -23 2.27 0.60
-1 2 -23 2.62 0.63
-2 -2 -23 12.68 1.17
-2 2 -23 11.81 1.10
-3 -2 -23 0.20 0.54
-3 2 -23 0.72 0.51
-4 -2 -23 0.61 0.58
-4 2 -23 1.71 0.61
4 -3 -23 2.72 0.69
-4 -3 23 4.35 0.70
4 3 -23 3.38 0.67
3 -3 -23 3.50 0.73
-3 -3 23 3.99 0.67
3 3 -23 4.92 0.76
3 3 -23 2.07 0.62
-2 -3 23 2.70 0.56
2 -3 -23 3.11 0.66
2 3 -23 2.72 0.62
2 3 -23 2.80 0.63
-1 -3 23 1.49 0.46
1 -3 -23 1.52 0.60
1 3 -23 1.65 0.58
1 3 -23 1.32 0.52
0 -3 23 2.72 0.51
0 -3 -23 0.92 0.52
0 3 -23 1.65 0.58
0 3 -23 2.24 0.58
-1 -3 -23 3.66 0.71
1 -3 23 3.83 0.53
-1 3 -23 3.86 0.69
-1 3 -23 3.05 0.67
-2 -3 -23 4.05 0.78
-2 3 -23 5.64 0.80
-3 -3 -23 6.93 0.95
-4 -3 -23 0.07 0.53
-3 -4 23 3.91 0.67
3 -4 -23 4.19 0.74
2 -4 -23 2.53 0.68
-2 -4 23 2.73 0.57
2 4 -23 2.26 0.61
-1 -4 23 0.99 0.41
1 -4 -23 0.00 0.49
1 4 -23 -0.04 0.49
0 -4 -23 8.09 0.98
0 -4 23 10.06 0.85
0 4 -23 7.36 0.93
-1 -4 -23 7.28 0.96
-1 4 -23 9.39 1.01
-2 -4 -23 0.48 0.53
-2 4 -23 -0.03 0.62
-3 -4 -23 1.27 0.64
-5 0 24 2.46 0.62
-4 0 24 1.29 0.51
3 0 -24 0.12 0.52
2 0 -24 5.34 0.84
1 0 -24 2.84 0.70
0 0 -24 0.44 0.48
-1 0 -24 0.45 0.49
-2 0 -24 3.27 0.70
-3 0 -24 -0.02 0.50
-4 0 -24 0.10 0.51
-4 -1 24 4.37 0.71
3 -1 -24 3.19 0.72
-3 -1 24 3.19 0.59
3 1 -24 2.95 0.71
-2 -1 24 3.06 0.56
2 -1 -24 2.26 0.71
2 1 -24 2.92 0.71
1 -1 -24 0.73 0.56
1 1 -24 1.71 0.66
0 -1 -24 5.64 0.83
0 1 -24 5.37 0.79
-1 -1 -24 15.74 1.23
-1 1 -24 15.38 1.20
-2 -1 -24 1.02 0.53
-2 1 -24 0.91 0.58
-3 -1 -24 2.31 0.68
-3 1 -24 3.79 0.83
-4 -1 -24 1.07 0.58
-4 1 -24 -0.34 0.49
4 -2 -24 0.70 0.60
-4 -2 24 0.51 0.47
3 -2 -24 8.53 1.07
-3 -2 24 8.25 0.86
3 2 -24 8.93 1.03
2 -2 -24 3.27 0.72
-2 -2 24 3.51 0.60
2 2 -24 3.83 0.71
-1 -2 24 5.49 0.70
1 -2 -24 5.73 0.87
1 2 -24 5.90 0.86
0 -2 24 3.43 0.56
0 -2 -24 2.65 0.64
0 2 -24 2.92 0.64
-1 -2 -24 4.07 0.75
1 -2 24 3.59 0.54
-1 2 -24 2.32 0.63
-2 -2 -24 0.49 0.51
-2 2 -24 0.21 0.50
-3 -2 -24 4.20 0.81
-3 2 -24 5.10 0.82
-4 -2 -24 6.20 0.96
-4 2 -24 4.23 0.82
-3 -3 24 4.98 0.75
3 -3 -24 4.14 0.83
3 3 -24 7.57 0.90
2 -3 -24 8.40 1.06
-2 -3 24 8.04 0.84
2 3 -24 7.44 0.89
2 3 -24 7.94 0.92
-1 -3 24 2.89 0.56
1 -3 -24 1.22 0.60
1 3 -24 3.12 0.68
1 3 -24 2.11 0.60
0 -3 24 6.92 0.73
0 -3 -24 7.49 0.96
0 3 -24 7.22 0.87
0 3 -24 8.22 0.92
1 -3 24 6.20 0.68
-1 -3 -24 5.06 0.84
-1 3 -24 5.86 0.82
-2 -3 -24 9.38 1.06
-3 -3 -24 4.78 0.83
-1 -4 24 0.92 0.47
1 -4 -24 1.04 0.56
0 -4 24 1.45 0.49
0 -4 -24 1.04 0.54
-1 -4 -24 5.68 0.88
3 0 -25 7.46 0.96
2 0 -25 3.70 0.75
1 0 -25 8.12 0.96
0 0 -25 0.75 0.48
-1 0 -25 2.51 0.67
-2 0 -25 5.49 0.89
-3 0 -25 14.53 1.27
-3 -1 25 1.27 0.52
3 -1 -25 1.86 0.68
3 1 -25 3.28 0.74
2 -1 -25 1.30 0.59
-2 -1 25 0.55 0.41
2 1 -25 1.42 0.59
1 -1 -25 5.77 0.91
1 1 -25 3.60 0.78
0 -1 -25 1.36 0.61
0 1 -25 1.03 0.57
-1 -1 -25 0.44 0.54
-1 1 -25 0.51 0.49
-2 -1 -25 -0.38 0.41
-2 1 -25 -0.19 0.47
-3 -1 -25 4.02 0.83
-3 1 -25 3.10 0.79
3 -2 -25 0.31 0.60
-3 -2 25 1.01 0.49
3 2 -25 1.03 0.59
2 -2 -25 1.34 0.66
-2 -2 25 0.30 0.44
2 2 -25 0.54 0.50
-1 -2 25 2.32 0.52
1 -2 -25 2.60 0.68
1 2 -25 2.60 0.65
0 -2 -25 -0.96 0.42
0 -2 25 0.04 0.40
0 2 -25 0.16 0.51
-1 -2 -25 6.69 0.93
1 -2 25 7.26 0.75
-1 2 -25 6.50 0.91
-2 -2 -25 2.00 0.62
-2 2 -25 0.98 0.61
-1 -3 25 6.69 0.77
1 -3 -25 5.69 0.88
1 3 -25 7.43 0.93
0 -3 -25 3.98 0.79
0 -3 25 4.77 0.67
0 3 -25 2.10 0.67
-1 -3 -25 0.72 0.56
2 0 -26 2.74 0.78
1 0 -26 -0.23 0.50
0 0 -26 0.56 0.58
-1 0 -26 5.20 0.81
2 -1 -26 1.06 0.66
-2 -1 26 0.13 0.41
2 1 -26 0.24 0.59
1 -1 -26 7.76 0.99
-1 -1 26 8.53 0.86
1 1 -26 7.36 0.99
0 -1 -26 2.80 0.65
0 1 -26 3.36 0.73
-1 -1 -26 3.80 0.76
-1 1 -26 2.44 0.68
0 0 0 0.00 0.00
;
_shelx_hkl_checksum 11647
_shelx_res_file
;
TITL GlyMet in P2(1)
shelx.res
created by SHELXL-2018/1 at 12:31:12 on 02-May-2023
CELL 0.71073 6.2517 5.4935 14.5686 90.000 91.147 90.000
ZERR 2.00 0.0002 0.0002 0.0006 0.000 0.004 0.000
LATT -1
SYMM -X, 0.5+Y, -Z
SFAC C H N O S
UNIT 14 28 4 6 2
L.S. 20
ACTA
CONF
EQIV $1 X+1, Y, Z
HTAB N1 O3_$1
HTAB N1 O1
EQIV $2 X+1, Y+1, Z
HTAB N1 O2_$2
EQIV $3 1-X, 1/2+Y, -Z
HTAB N1 O3_$3
EQIV $4 X, Y+1, Z
HTAB N2 O2_$4
BOND $H
FMAP 2
PLAN 5
SIZE 0.03 0.29 0.38
TEMP -183
WGHT 0.041700
FVAR 0.47779
S1 5 -0.201455 0.444743 0.428480 11.00000 0.01416 0.01407 =
0.01605 -0.00091 0.00637 -0.00108
O1 4 0.693104 0.519624 0.162783 11.00000 0.01174 0.00766 =
0.02158 0.00160 0.00359 0.00107
O2 4 0.192512 0.156878 0.172870 11.00000 0.01141 0.00719 =
0.01700 -0.00063 -0.00090 -0.00059
O3 4 0.178531 0.508956 0.095971 11.00000 0.01443 0.01117 =
0.00999 0.00052 -0.00093 0.00163
N1 3 0.878801 0.899357 0.083547 11.00000 0.00938 0.00877 =
0.01184 0.00106 0.00074 -0.00089
H11N 2 0.912857 0.757137 0.094825 11.00000 -1.50000
H12N 2 0.980793 0.993524 0.107232 11.00000 -1.50000
H13N 2 0.865057 0.912203 0.025654 11.00000 -1.50000
N2 3 0.422471 0.735845 0.225782 11.00000 0.00872 0.00685 =
0.01333 0.00057 0.00075 -0.00082
H2N 2 0.352592 0.862899 0.217070 11.00000 -1.20000
C1 1 0.670908 0.943994 0.127516 11.00000 0.01188 0.00790 =
0.01992 0.00239 0.00502 0.00054
AFIX 23
H1D 2 0.563279 0.995080 0.080609 11.00000 -1.20000
H1E 2 0.686342 1.076254 0.173329 11.00000 -1.20000
AFIX 0
C2 1 0.597159 0.712582 0.174247 11.00000 0.00852 0.00742 =
0.01214 0.00026 -0.00089 -0.00116
C3 1 0.308745 0.516541 0.251722 11.00000 0.00863 0.00766 =
0.01041 0.00136 0.00011 -0.00090
AFIX 13
H3 2 0.410296 0.406010 0.285399 11.00000 -1.20000
AFIX 0
C4 1 0.220802 0.383113 0.165872 11.00000 0.00684 0.00759 =
0.01065 -0.00061 0.00106 0.00063
C5 1 0.125226 0.584603 0.316033 11.00000 0.01207 0.01038 =
0.01098 -0.00066 0.00213 -0.00130
AFIX 23
H5A 2 0.184307 0.675550 0.369448 11.00000 -1.20000
H5B 2 0.023082 0.692558 0.282903 11.00000 -1.20000
AFIX 0
C6 1 0.006777 0.359986 0.349914 11.00000 0.01413 0.01131 =
0.01421 -0.00034 0.00536 -0.00113
AFIX 23
H6A 2 0.109333 0.249024 0.381309 11.00000 -1.20000
H6B 2 -0.057507 0.272165 0.296822 11.00000 -1.20000
AFIX 0
C7 1 -0.328586 0.151363 0.438122 11.00000 0.01472 0.01832 =
0.01944 0.00250 0.00299 -0.00458
AFIX 137
H7A 2 -0.381335 0.098919 0.377488 11.00000 -1.50000
H7B 2 -0.448752 0.163281 0.480064 11.00000 -1.50000
H7C 2 -0.224743 0.032488 0.462053 11.00000 -1.50000
AFIX 0
HKLF 4
REM GlyMet in P2(1)
REM R1 = 0.0332 for 5356 Fo > 4sig(Fo) and 0.0399 for all 5922 data
REM 131 parameters refined using 1 restraints
END
WGHT 0.0417 0.0000
REM Highest difference peak 0.532, deepest hole -0.303, 1-sigma level 0.065
Q1 1 0.2024 0.4447 0.1311 11.00000 0.05 0.53
Q2 1 -0.1917 0.4641 0.4808 11.00000 0.05 0.45
Q3 1 0.2893 0.4533 0.2063 11.00000 0.05 0.43
Q4 1 0.6243 0.8267 0.1479 11.00000 0.05 0.40
Q5 1 0.1812 0.2822 0.1822 11.00000 0.05 0.38
;
_shelx_res_checksum 74456
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S S1 -0.20146(4) 0.44474(6) 0.42848(2) 0.01468(6) Uani d 1 . .
O O1 0.69310(13) 0.51962(16) 0.16278(6) 0.01361(15) Uani d 1 . .
O O2 0.19251(13) 0.15688(15) 0.17287(6) 0.01189(14) Uani d 1 . .
O O3 0.17853(13) 0.50896(16) 0.09597(6) 0.01188(13) Uani d 1 . .
N N1 0.87880(15) 0.89936(16) 0.08355(7) 0.00999(15) Uani d 1 . .
H H11N 0.913(3) 0.757(4) 0.0948(13) 0.015 Uiso d 1 . .
H H12N 0.981(3) 0.994(4) 0.1072(12) 0.015 Uiso d 1 . .
H H13N 0.865(3) 0.912(4) 0.0257(13) 0.015 Uiso d 1 . .
N N2 0.42247(14) 0.73584(17) 0.22578(7) 0.00962(14) Uani d 1 . .
H H2N 0.353(3) 0.863(4) 0.2171(13) 0.012 Uiso d 1 . .
C C1 0.67091(16) 0.9440(2) 0.12752(8) 0.01317(16) Uani d 1 . .
H H1D 0.563279 0.995080 0.080609 0.016 Uiso calc 1 . .
H H1E 0.686342 1.076254 0.173329 0.016 Uiso calc 1 . .
C C2 0.59716(16) 0.71258(19) 0.17425(7) 0.00938(15) Uani d 1 . .
C C3 0.30874(16) 0.51654(19) 0.25172(7) 0.00890(15) Uani d 1 . .
H H3 0.410296 0.406010 0.285399 0.011 Uiso calc 1 . .
C C4 0.22080(16) 0.38311(18) 0.16587(7) 0.00835(15) Uani d 1 . .
C C5 0.12523(18) 0.5846(2) 0.31603(8) 0.01112(17) Uani d 1 . .
H H5A 0.184307 0.675550 0.369448 0.013 Uiso calc 1 . .
H H5B 0.023082 0.692558 0.282903 0.013 Uiso calc 1 . .
C C6 0.00678(19) 0.3600(2) 0.34991(8) 0.01315(18) Uani d 1 . .
H H6A 0.109333 0.249024 0.381309 0.016 Uiso calc 1 . .
H H6B -0.057507 0.272165 0.296822 0.016 Uiso calc 1 . .
C C7 -0.3286(2) 0.1514(2) 0.43812(9) 0.0175(2) Uani d 1 . .
H H7A -0.381335 0.098919 0.377488 0.026 Uiso calc 1 . .
H H7B -0.448752 0.163281 0.480064 0.026 Uiso calc 1 . .
H H7C -0.224743 0.032488 0.462053 0.026 Uiso calc 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
S1 0.01416(11) 0.01407(11) 0.01605(12) -0.00108(10) 0.00637(8) -0.00091(10)
O1 0.0117(3) 0.0077(3) 0.0216(4) 0.0011(3) 0.0036(3) 0.0016(3)
O2 0.0114(3) 0.0072(3) 0.0170(4) -0.0006(2) -0.0009(3) -0.0006(3)
O3 0.0144(3) 0.0112(3) 0.0100(3) 0.0016(3) -0.0009(2) 0.0005(3)
N1 0.0094(3) 0.0088(4) 0.0118(4) -0.0009(3) 0.0007(3) 0.0011(3)
N2 0.0087(3) 0.0068(3) 0.0133(4) -0.0008(3) 0.0007(3) 0.0006(3)
C1 0.0119(4) 0.0079(3) 0.0199(4) 0.0005(4) 0.0050(3) 0.0024(4)
C2 0.0085(4) 0.0074(3) 0.0121(4) -0.0012(3) -0.0009(3) 0.0003(3)
C3 0.0086(3) 0.0077(3) 0.0104(4) -0.0009(3) 0.0001(3) 0.0014(3)
C4 0.0068(3) 0.0076(3) 0.0107(4) 0.0006(3) 0.0011(3) -0.0006(3)
C5 0.0121(4) 0.0104(4) 0.0110(4) -0.0013(3) 0.0021(3) -0.0007(3)
C6 0.0141(4) 0.0113(4) 0.0142(4) -0.0011(3) 0.0054(3) -0.0003(3)
C7 0.0147(5) 0.0183(5) 0.0194(5) -0.0046(4) 0.0030(4) 0.0025(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C7 S1 C6 . . 98.22(6) ?
C1 N1 H11N . . 107.2(13) ?
C1 N1 H12N . . 111.5(12) ?
H11N N1 H12N . . 107.1(19) ?
C1 N1 H13N . . 110.1(12) ?
H11N N1 H13N . . 107.3(19) ?
H12N N1 H13N . . 113.3(18) ?
C2 N2 C3 . . 118.29(9) ?
C2 N2 H2N . . 115.1(13) ?
C3 N2 H2N . . 118.5(13) ?
N1 C1 C2 . . 109.41(9) ?
N1 C1 H1D . . 109.8 ?
C2 C1 H1D . . 109.8 ?
N1 C1 H1E . . 109.8 ?
C2 C1 H1E . . 109.8 ?
H1D C1 H1E . . 108.2 ?
O1 C2 N2 . . 124.15(10) ?
O1 C2 C1 . . 120.47(9) ?
N2 C2 C1 . . 115.37(9) ?
N2 C3 C4 . . 110.59(8) ?
N2 C3 C5 . . 109.33(9) ?
C4 C3 C5 . . 110.53(8) ?
N2 C3 H3 . . 108.8 ?
C4 C3 H3 . . 108.8 ?
C5 C3 H3 . . 108.8 ?
O3 C4 O2 . . 125.57(10) ?
O3 C4 C3 . . 117.55(9) ?
O2 C4 C3 . . 116.86(9) ?
C6 C5 C3 . . 111.85(9) ?
C6 C5 H5A . . 109.2 ?
C3 C5 H5A . . 109.2 ?
C6 C5 H5B . . 109.2 ?
C3 C5 H5B . . 109.2 ?
H5A C5 H5B . . 107.9 ?
C5 C6 S1 . . 110.86(8) ?
C5 C6 H6A . . 109.5 ?
S1 C6 H6A . . 109.5 ?
C5 C6 H6B . . 109.5 ?
S1 C6 H6B . . 109.5 ?
H6A C6 H6B . . 108.1 ?
S1 C7 H7A . . 109.5 ?
S1 C7 H7B . . 109.5 ?
H7A C7 H7B . . 109.5 ?
S1 C7 H7C . . 109.5 ?
H7A C7 H7C . . 109.5 ?
H7B C7 H7C . . 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
S1 C7 . 1.8037(13) ?
S1 C6 . 1.8114(11) ?
O1 C2 . 1.2310(13) ?
O2 C4 . 1.2598(13) ?
O3 C4 . 1.2546(13) ?
N1 C1 . 1.4809(14) ?
N1 H11N . 0.83(2) ?
N1 H12N . 0.886(19) ?
N1 H13N . 0.849(19) ?
N2 C2 . 1.3437(14) ?
N2 C3 . 1.4527(14) ?
N2 H2N . 0.832(19) ?
C1 C2 . 1.5181(16) ?
C1 H1D . 0.9900 ?
C1 H1E . 0.9900 ?
C3 C4 . 1.5415(15) ?
C3 C5 . 1.5417(15) ?
C3 H3 . 1.0000 ?
C5 C6 . 1.5262(16) ?
C5 H5A . 0.9900 ?
C5 H5B . 0.9900 ?
C6 H6A . 0.9900 ?
C6 H6B . 0.9900 ?
C7 H7A . 0.9800 ?
C7 H7B . 0.9800 ?
C7 H7C . 0.9800 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N1 H11N O3 1_655 0.83(2) 2.15(2) 2.8513(13) 143.0(18) yes
N1 H11N O1 . 0.83(2) 2.15(2) 2.6619(13) 120.1(16) yes
N1 H12N O2 1_665 0.886(19) 1.850(19) 2.7275(12) 170.7(18) yes
N1 H13N O3 2_655 0.849(19) 1.86(2) 2.7006(13) 168(2) yes
N2 H2N O2 1_565 0.832(19) 2.000(19) 2.8225(12) 170.0(18) yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C3 N2 C2 O1 . . . . -15.40(16) ?
C3 N2 C2 C1 . . . . 163.44(9) ?
N1 C1 C2 O1 . . . . -8.46(15) ?
N1 C1 C2 N2 . . . . 172.66(9) ?
C2 N2 C3 C4 . . . . -62.19(12) ?
C2 N2 C3 C5 . . . . 175.89(9) ?
N2 C3 C4 O3 . . . . -27.75(13) ?
C5 C3 C4 O3 . . . . 93.47(11) ?
N2 C3 C4 O2 . . . . 153.99(9) ?
C5 C3 C4 O2 . . . . -84.80(11) ?
N2 C3 C5 C6 . . . . -176.94(9) ?
C4 C3 C5 C6 . . . . 61.10(12) ?
C3 C5 C6 S1 . . . . 177.94(8) ?
C7 S1 C6 C5 . . . . 171.26(9) ?